Triethylamine → 4-[(2-Sulfamoyl-5-thienyl)sulfonyl]phenyl 1-acetylpiperidine-4-carboxylate

HRID 1632742

반응식

HRID 1632742 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:11]2[S:15][C:14]([S:16]([NH2:19])(=[O:18])=[O:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl.[C:28]([N:31]1[CH2:36][CH2:35][CH:34]([C:37](Cl)=[O:38])[CH2:33][CH2:32]1)(=[O:30])[CH3:29]>CC(C)=O>[C:28]([N:31]1[CH2:32][CH2:33][CH:34]([C:37]([O:1][C:2]2[CH:7]=[CH:6][C:5]([S:8]([C:11]3[S:15][C:14]([S:16](=[O:17])(=[O:18])[NH2:19])=[CH:13][CH:12]=3)(=[O:9])=[O:10])=[CH:4][CH:3]=2)=[O:38])[CH2:35][CH2:36]1)(=[O:30])[CH3:29]

참가 물질

5

반응물 3

HCID 8471Triethylamine3회HCID 127368925-(4-Hydroxyphenyl)sulfonylthiophene-2-sulfonamideHCID 534308101-Acetylpiperidine-4-carbonyl chloride hydrochloride2회

생성물 1

HCID 204423674-[(2-Sulfamoyl-5-thienyl)sulfonyl]phenyl 1-acetylpiperidine-4-carboxylate

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 5-[(4-hydroxyphenyl)sulfonyl]thiophene-2-sulfonamide (3.19 g; 0.01 mole) in acetone (60 ml) at -15° was treated with triethylamine (1.11 g; 0.011 mole). Then 1-acetylpiperidine-4-carbonyl chloride hydrochloride (2.41 g; 0.011 mole) was added, portionwise, during 15 minutes at -15°. The cooling bath was removed and stirring was continued. After 20 hours at room temperature, the reaction mixture was treated with triethylamine (1.11 g; 0.011 mole). Then after stirring one hour longer, the reaction mixture was treated with 1-acetylpiperidine-4-carbonyl chloride hydrochloride (2.41 g; 0.011 mole) and triethylamine (2.22 g; 0.022 mole) and stirred at room temperature.

후처리

  1. customThe cooling bath was removed
  2. waitAfter 20 hours at room temperature
  3. stirringThen after stirring one hour longer
  4. stirringstirred at room temperature

출처 및 근거

ORD 기록
ord-d259bbaad2a743b2b218fca536653630
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04477466

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